HRID1995026

反应详情

EQUATION

反应方程式

HRID 1995026 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

42.0 g 6-Hydroxy-4-methyl-2-n-hexylamino-pyrimidin (0.2 Mol), 27.6 g K2CO3 (0.2 Mol), 24.4 g 2,3-dichloro-1-propene (0.22 Mol) and 150 ml dimethylformamide are charged in a sulphonation flask. The mixture is heated for about 3 hours at a bath temperature of 110°, then cooled to room temperature and thereafter poured in 500 ml water. This mixture is extracted with ether, the ether extract dried with Na2SO4 and concentrated with the aid of a flask rotary vacuum evaporator at a temperature of up to 60°. The impure title compound is obtained as a brown oil, which is purified chromatographically with ether/hexane 1:3 on silicagel to give a yellow oil that slowly crystallises. m.p. 36°-37°.

WORKUP

后处理

  1. temperatureThe mixture is heated for about 3 hours at a bath temperature of 110°
  2. extractionThis mixture is extracted with ether
  3. extractionthe ether extract
  4. dry with materialdried with Na2SO4
  5. concentrationconcentrated with the aid of a flask
  6. customrotary vacuum evaporator at a temperature of up to 60°